Hydrochloric Acid → 4-Formyl-3-hydroxyphenyl acetate

HRID 2369828ノート

反応式

HRID 2369828 の反応式
[C:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([CH:11]=[O:12])=[C:7]([O:13]C(=O)C)[CH:6]=1)(=[O:3])[CH3:2].[OH-].[Na+].Cl>C(O)C.O.C(OCC)(=O)C>[C:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([CH:11]=[O:12])=[C:7]([OH:13])[CH:6]=1)(=[O:3])[CH3:2]

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 11127858HCID 11127858、化合物

生成物 1

HCID 126480914-Formyl-3-hydroxyphenyl acetate収率 44.5%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 4-formylbenzene-1,3-diyl diacetate (5.56 g, 25.08 mmol) in ethanol (20 mL) was added a solution of sodium hydroxide (1.00 g, 25.08 mmol) in water (12 mL). The reaction was stirred overnight at room temperature. The reaction was carefully neutralized with 2.0 N aqueous solution of hydrochloric acid (12.8 mL) at 0° C. and diluted with ethyl acetate (400 mL). The organic layer was washed with water (60 mL) and saturated aqueous sodium chloride (50 mL), dried over magnesium sulfate, filtered, and concentrated to afford, the product (2.01 g, 44% yield) as a gray solid: 1H NMR (400 MHz, d-MeOH): δ 9.90 (s, 1H), 7.68 (d, 1H), 6.80 (d, 1H), 6.75 (s, 1H), 4.82 (br s, 1H), 2.20 (s, 3H).

後処理

  1. washThe organic layer was washed with water (60 mL) and saturated aqueous sodium chloride (50 mL)
  2. dry with materialdried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customto afford

出典と根拠

ORDレコード
ord-2c2c921313354294946711a8f50c7eb3
出典データセット
uspto-grants-2014_04
特許番号
US08710038B2

反応ノート

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